Materials Sciences and Applications, 2013, 4, 723-729
Published Online November 2013 (http://www.scirp.org/journal/msa)
http://dx.doi.org/10.4236/msa.2013.411091
Open Access MSA
723
Investigation on the Microstructure and Electrical
Properties of the Compositionally Modified PZT Ceramics
Prepared by Mixed-Oxide Method
Malika Abba, Ahmed Boutarfaia, Zelikha Necira, Noura Abdessalem, Hayet Menasra,
Abdelhek Meklid
Laboratory of Applied Chemistry, Department of Science Matter, University of Biskra, Biskra, Algeria.
Received August 17th, 2013; revised September 29th, 2013; accepted October 16th, 2013
Copyright © 2013 Malika Abba et al. This is an open access article distributed under the Creative Commons Attribution License,
which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
ABSTRACT
The structural and electrical properties of Pb[ZrxTi0.95−x(Mo1/3In2/3)0.05]O3 piezoelectric ceramics system with the com-
position near the morphotropic phase boundary were investigated as a function of the Zr/Ti ratio. Studies were per-
formed on the samples prepared by the conventional method of thermal synthesis of mixed oxides. The materials struc-
ture was investigated by X-ray diffractometry to demonstrate the co-existence of the tetragonal and rhombohedral
phases. In the present system, the MPB, in which the tetragonal and rhombohedral phases coexist, is in a composition
range of 0.47 ≤ x ≤ 0.50. The lattice constants of the a and c axes for the samples were calculated from the XRD patterns.
Microstructure of the sintered ceramics was observed by scanning electron microscopy (SEM) of free surfaces speci-
mens. The relative permittivity, dielectric dissipation, piezoelectric coefficient and electromechanical coupling factor
reach at maximum value x = 0.49 (εr = 7300.345 (at the Curie temperature), tanδ = 0.002050, d31 = 94.965 PC/N and kp
= 0.513 and a Curie temperature of 430˚C). These properties are very promising for applications in ultrasonic motors.
Keywords: Morphotropic Phase Boundary; Sintering Temperature; Zr/Ti Ratio
1. Introduction
Lead zirconate titanate Pb(Zr,Ti)O3, a solid solution of
perovskite ferroelectric PbTiO3 and anti-ferroelectric
PbZrO3 with different Zr/Ti ratio, is an important mate-
rial that is widely used in electronic sensors, actuators,
resonators and filters [1-3]. The materials with a per-
ovskite structure of general formula ABO3 (where A =
mono or divalent ions, B = tri, tetra or pentavalent ions)
have been found to be very useful and interesting for
different solid-state devices [4-8]. By making suitable
substitution at A and/or B-site of ABO3 structure, a large
number of charge neutral or deficient compounds have
been prepared [9-11] which have been found to be very
suitable and useful for many industrial applications.
In order to satisfy the requirements of practical appli-
cations of ultrasonic motors, many ternary and quater-
nary solid-solutions such as: Pb(Mn1/3Nb2/3)O3-PZT,
Pb(Mn1/3Sb2/3)O3-PZT,Pb(Cd1/3Nb2/3)O3-PZT,
Pb(Mn1/3Nb2/3)(Ni1/3Nb2/3)O3-PZT, have been synthesized
by the modification or the substitution [12-18].
The influence of technological factors on the width of
the co-existence region was investigated on the ternary
system Pb[Zrx,Ti(0,95−x)(Mo1/3,In2/3)0.05]O3 by X-ray dif-
fraction by varying the ratio Zr/Ti. The purpose of this
work is to study the influence of sintering temperature on
density, porosity and grain size on the ceramic in order to
determine the width of co-existence of tetragonal and
rhombohedral phases and the exact composition of the
MPB rather than to determine the dielectric and the pie-
zoelectric properties of these ceramics near the MPB in
detail.
2. Experimental
All of the specimens were prepared by the conventional
ceramics technologie. The compositions of the
Pb[Zrx,Ti(0.95−x)(Mo1/3,In2/3)0.05]O3 system werewith 46 ≤ x
≤ 55. The commercially available PbO, ZrO2, TiO2,
MoO3 and In2O3, were used as the raw materials. Mixed
oxides, after milling, were calcined at 800˚C for 2 h at
heating and cooling rates of 2˚C/min. After calcinations,

Investigation on the Microstructure and Electrical Properties of the Compositionally Modified
PZT Ceramics Prepared by Mixed-Oxide Method
724
the ground and milled powders were pressed into disks
13 mm in diameter and about 1 mm in thickness. Pressed
disks of 3PbO + 2ZrO2 placed in a capped crucible to pre-
vent PbO evaporation during sintering. Four sintering con-
ditions were selected to be used with both methods rang-
ing 1000˚C, 1100˚C, 1150˚C, 1180˚C and 1200˚C for 2 h.
The crystal structure of the samples was analyzed us-
ing X-ray diffractometry (XRD; Siemens D500). The
voltage and currents ratings used were 40 kV, 30 mA
respectively, and CuKα radiation was used. The dif-
fraction data were collected with X-ray scan speed of
0.1˚·min−1. The bulk density was measured using the
Archimedes method.
To investigate the electrical properties, the electrodes
were made by applying a silver paste on the two major
faces of the sintered disks followed by heat treatment at
750˚C for thirty minutes. The dielectric constant ε was
calculated from the capacitance at a frequency of one
KHz. It was measured at temperature ranging from 25˚C
to 400˚C with a heating rate of one ˚C/minute by using
an impedance analyzer (HP4192A, Heweltt-Packard).
The piezoelectric samples firstly were being poled in a
silicone oil bath at 120˚C by applying a d.c. field of thirty
KV/cm for thirty minutes; and, then, were being cold
under the same electric field.
They were aged for twenty-four hours before testing.
The electromechanical coupling factor Kp was deter-
mined by the resonance and anti-resonance technique
from the “Equation (1)” [19].
()
12
22
2
2.51
2
ar
p
a
ff
Kf

×−

=


(1)
fa: anti-resonant frequency (Hz).
fr: resonant frequency (Hz).
3. Results and Discussion
3.1. Phase Structure
The sintered powders were examined by X-ray diffrac-
tometry to ensure phase purity and to identify the phases.
The phases of the samples were detected using XRD (at
room temperature) for several compositions given in Ta-
ble 1.
It is reported that tetragonal, rhombohedral and T-R
phases were identified by an analysis of the peaks 0 0 2
(tetragonal), 2 0 0 (tetragonal), 2 0 0 (rhombohedral)) in
the 2
θ range 43˚ - 47˚.
The splitting of (0 0 2) and (2 0 0) peaks indicates that
they are the ferroelectric tetragonal phase (T), while the
single (2 0 0) peak shows the rhombohedral phase (R)
Figure 1 [20].
Triplet peaks indicate that the sample consists of a
Table 1. Series of compositions and crystal structure.
Crystal structure
Sample 1000˚C 1100˚C 1150˚C 1180˚C
Pb[Zr0.46Ti 0.49(Mo1/3In2/3)0.05]O3 T T T T
Pb[Zr0.47Ti 0.48(Mo1/3In2/3)0.05]O3 T + R T T T + R
Pb[Zr0.49Ti 0.46(Mo1/3In2/3)0.05]O3 T + R T + R T + RT + R
Pb[Zr0.50Ti 0.45(Mo1/3In2/3)0.05]O3 T + R T + R T + RT + R
Pb[Zr0.51Ti 0.44(Mo1/3In2/3)0.05]O3 T + R T + R T + RR
Pb[Zr0.52Ti 0.43(Mo1/3In2/3)0.05]O3 T + R T + R T + RR
Pb[ Zr0.54Ti 0.41(Mo1/3In2/3)0.05]O3T + R T + R R R
Pb[Zr0.55Ti 0.40(Mo1/3In2/3)0.05]O3 R R R R
T = Tetragonal; R = Rhombohedral; T-R = Tetragonal-Rhombohedral.
Figure 1. The XRD patterns of Pb
[Zrx,Ti(0.95−x)(Mo1/3,In2/3)0.05]O3 systemwith 0.46 ≤ x ≤ 0.55.
mixture of tetragonal and rhombohedral phases. The
multiple peak separation method was used to estimate the
relative fraction of coexisting phases by which the rela-
tive phase fraction MR and MT were then calculated using
the following Equations (2) and (3) [21]:
()
() () ()
200
200 002 200
R
R
RTT
I
MIII =++ (2)
() ()
() () ()
200 002
200 002 200
TT
T
RTT
II
MIII
+
++
= (3)
It is clear that, IR(200) is the integral intensity of the
(200) reflection of the rhombohedral phase and IT(200),
IT(002) are the integral intensities of the (200) and (002)
reflections of the tetragonal phase, respectively. A transi-
tion from tetragonal to rhombohedral phase is observed
as Zr/Ti ratio increases. With increasing Zr/Ti ratio,
tetragonal relative fraction decreases and rhombohedral
relative fraction increases.
At 1180˚C Figure 2, it is shown that the tetragonal
structure can be formed up to xT > 0.46, while the rhom-
bohedral structure becomes stabilized for xR < 0.51.
However, at x = 0.46 - 0.51 tetragonal and rhombohedral
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Investigation on the Microstructure and Electrical Properties of the Compositionally Modified
PZT Ceramics Prepared by Mixed-Oxide Method
725
Figure 2. Variation of the relative content of the tetragonal
and rhombohedral phases with different Zr% in the
Pb[ZrxTi0,95−x(Mo1/3In2/3)0.05]O3 (for a sintering temperature
about 1180˚C) [20].
phases coexist. The co-existence region is therefore quite
narrow (Δx ≈ 0.05) and extends between xT and xR. The
width Δx = xT − xR of the co-existence region from our
work is close to that obtained by others [22,23]. The co-
existence of tetragonal and rhombohedral phases has,
therefore, to be attributed to the first order nature of the
MPB, this is marked contrast to the proposition of Kake-
gawa and al. [24,25] that the coexistence is invariably
due to compositional fluctuations.
The study of density is necessary to optimize the op-
timum sintering temperature. The quality of the material
increases with the increase of density and it increases
with the increase of the sintering temperature [26]. The
optimum temperature for sintering is determined from
the pattern density as a function of sintering temperature
d = f(T). So, the maximum density is the product of bet-
ter quality electrical (low dielectric loss). Figure 3 gath-
ers the curves of the density of all samples depending on
the sintering temperature. A similar shape for all curves
is that: the density is minimal for a sintering temperature
T = 1000˚C, it begins to grow until it reaches a maximum
value at a sintering temperature T = 1180˚C. Then, it
decreases at the sintering temperature T = 1200˚C which
means that the optimum temperature for sintering is
1180˚C. The increased density means fewer and pore size,
so the volume of the cell decreases and consequently the
structure becomes more compact.
The optimum sintering temperature depends on several
factors such as the addition of impurities, the rate of
heating, time of thermal treatment and protecting atmos-
phere.
Changes in the density of different samples of
Pb[ZrxTi0,95−x(Mo1/3In2/3)0.05]O3 sintered at 1180˚C de-
pending on the rate of Zr is shown in Figure 4.
The shape of the curve shows that the density increases
with the increase of Zr concentration until a maximum
Figure 3. Effect of sintering temperature on density for
Pb[ZrxTi0,95−x(Mo1/3In2/3)0.05]O3.
Figure 4. Evolution of density as a function of the concen-
tration of Zr% [20].
value of 7.61g/cm3 (94.18% of theoretical density) at Zr =
49% (sample No. 3) and then it decreases [20].
Figure 5 shows the variation of the porosity for dif-
ferent samples depending on the concentration of Zr%
and the sintering temperature of 1180˚C, noting that the
porosity decreases until itreaches the minimum value p =
5.81% for Zr = 0.49 (sample No. 3) and then it increases.
The parameters of the lattice were determined from the
triplets (200) by using a nonlinear least squares method
[27]. The aR—parameter of the rhombohedral phase and
the aT—parameter, cT—parameter, and the tetragonality
(cT/aT) of the tetragonal phase of
Pb[ZrxTi0,95−x(Mo1/3In2/3)0.05]O3 ceramics are plotted as a
function of the ratio of Zr/Ti in Figure 6. The results
showed that the parameters of the lattice of the tetra-
gonalphase changed when the ratio of Zr/Ti was modi-
fied. While the value of the aT parameter increased, the
one of cT parameter decreased and the aR parameter of
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Investigation on the Microstructure and Electrical Properties of the Compositionally Modified
PZT Ceramics Prepared by Mixed-Oxide Method
726
Figure 5. The variation of porosity as a function of the con-
centration of Zr% for Pb [ZrxTi0.95−x(Mo1/3In2/3)0.05]O3 (for a
sintering temperature about 1180˚C) [20].
Figure 6. The parameters of the lattice of
Pb[ZrxTi0,95−x(Mo1/3In2/3)0.05]O3 ceramics as a function of
composition(for a sintering temperature about 1180˚C) [20].
the rhombohedral phase increased. The resulting values
of the parameters of the lattice of the tetragonal phase
showed that the cT/aT axial ratio is decreased as aT it is
increased and cT is decreased. The values of the parame-
ters of the lattice were revealed to be practically the same
as those which previously studied [28,29].
Figure 7 gives the SEM micrographs of free surfaces
of the specimens sintered at 1000˚C - 1180˚C for 2 h.
From these images, small crystallites with large pores for
specimens sintered at 1000˚C Figure 7(a) were noticed.
As the sintering temperature increased, the grain grew
and the average grain size increased slightly. Whereas,
the number and the size of the pores is decreased. The
grain size exponentially increased with the increase of
temperature and this can be well explained by the phe-
nomenological kinetic grain grow equation [30]. The
average grain size is 1.15 µm at temperature 1000˚C
which increases to 1.56 µm at temperature 1180˚C [20].
Figure 7. SEM micrographs for
Pb[Zr0.50Ti0.45(Mo1/3,In2/3)0.05]O3 ceramics sintered at (a)
1000˚C, (b) 1100˚C (c) 1150˚C and (d) 1180˚C.
3.2. Dielectric and Piezoelectric Properties
The dielectric properties at room temperature are plotted
as a function of the Zr/Ti ratio in Figure 8. The ε in-
crease with the increase of Zr/Ti ratio. It achieves a
maximum value of 1331.955 only when x = 0.49 and
then it decreases significantly as the Zr/Ti ratio increases
further. The tanδ shows an inverse trend and reaches the
minimum value of 0.00205 when x = 0.49.
The temperature dependence of the dielectric constant
for Pb[ZrxTi0.95−x(Mo1/3In2/3)0.05]O 3 ternary ceramics at 1
KHz is shown in Figure 9. It is observed in all the com-
positions as the temperature increase, the value of dielec-
tric constant increases and passes through a maximum (at
TC) and then decreases. The Curie temperature increased
from 340˚C to 440˚C in our choosing composition. The
maximum dielectric constant at MPB (x = 0.49) is about
7300.345.
The variation in dielectric constant with frequency for
Pb[ZrxTi0.95−x(Mo1/3In2/3)0.05]O3 ternary ceramics is shown
in Figure 10. The plots show that the dielectric constant
decreases with an increase in frequency, showing disper-
sion in lower frequency rang. It attains a constant value
and remains independent of frequency. Thereafter, all the
samples reveal dispersion due to Maxwell-Wagner [31,
32] type interfacial polarization in agreement with Koop’s
phenomenological theory [33]. The high value of dielec-
tric constant observed at lower frequencies can be ex-
plained on the basis of space charge polarization due to
heterogeneous in structure like impurities, porosity and
grain structure [34].
The electromechanical coupling factor (kp) and the
piezoelectric coefficient (d31) are shown in Figure 11.
These properties were also strongly influenced by the
composition of the specimen. The highest d31 of 94.965
pC/N and Kp of 0.513 were observed for the composition
of x = 0.49. Considering that the fact of this composition
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Investigation on the Microstructure and Electrical Properties of the Compositionally Modified
PZT Ceramics Prepared by Mixed-Oxide Method
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Figure 8. The dielectric constant ε and the loss tangent (at
room temperature, 1 KHz) for
Pb[ZrxTi0,95−x(Mo1/3In2/3)0.05]O3 ceramics sintered at 1180˚C.
Figure 9. Temperature dependence of the dielectric con-
stant for Pb[ZrxTi0.95−x(Mo1/3In2/3)0.05]O3 ceramics sintered
at 1180˚C (1 KHz).
Figure 10. Variation of dielectric constant with frequen-
cy for Pb[ZrxTi0,95−x(Mo1/3In2/3)0.05]O3 ceramics sintered at
1180˚C.
Figure 11. Variation of Kp and d31 for
Pb[ZrxTi0.95−x(Mo1/3In2/3)0.05]O3 ceramics sintered at 1180˚C.
corresponds to the MPB and the maximum piezoelectric
properties observed for this polycrystalline composition
are reasonable. When the PZT content was varied away
from the MPB, both the d31 and kp value decreased
asymmetrically. In the rhombohedral side, both the d31
and kp value were decreased much more rapidly.
4. Conclusions
In this study, ceramics in the
Pb[ZrxTi0.95−x(Mo1/3In2/3)0.05]O3 system (with 0.46 ≤ x ≤
0.55) were successfully prepared by a solid-state mixed-
oxide technique. The co-existence region was investi-
gated by X-ray diffraction. The study of the morpho-
tropic phase boundary has established that the phase
transition from tetragonal to rhombohedral symmetry
takes place at x = 0.49 and the width of the phase bound-
ary that has been found to be in the range of 0.47 ≤ x ≤
0.50 at 1180˚C.
The lattice parameters aT and cT of the tetragonal struc-
ture and aR of the rhombohedral structure were found to
change with composition. The effect of the sintering
temperature on the density and grain size has been inves-
tigated. It was demonstrated that the grain size and the
density increased with the increase of the sintering tem-
perature. The optimum sintering temperature (1180˚C)
corresponds to the maximum density. So, the minimum
value of porosity is also corresponds to the better quality
product.
The electrical and piezoelectric properties exhibit a
compositional dependence. The samples showing the co-
existence of morphotropic phase boundary (MPB) ex-
hibit good properties. The results indicate that although
this kind of ceramics displays good properties, further
study is needed to improve their stabilities of the ceramics
in order to be utilized in various temperature environ-
ments.
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